DE19803551C1 - Sample cell for microscopic investigation under conditions of high pressure, combined with extreme heating or cooling - Google Patents

Abstract

The cell is mounted on the slide stage of a commercially available microscope. It resists high pressures, the optical window (i) being adhered to a seat (k) held by a recessed ring nut (l). A self-bracing annular metal seal is included. Sample change is achieved via a separately sealed insertion opening (h), without dismantling the window assembly. Preferred features: The cell body is high tensile steel. There is a second window opposite the first; both comprising sapphire or diamond. For polarization microscopy investigations, the sample is placed between two crossed polarization films, and brought together with them into the tempering cell, via the insertion opening.

Description

The invention relates to a temperature cell for heating or cooling one with Microscope to be examined sample with the features of the preamble of claim 1.

Such a temperature control cell is known from the publication [1], but is for higher pressures not suitable. A pressure chamber suitable for higher pressures is known from the publication [2] known, however, this is designed exclusively for cooling purposes and would expand their functionality on heating purposes do not work reliably and at the same time be easy to use.

The invention is therefore based on the object of being easy to use and reliable Functioning heatable or coolable, high pressure resistant temperature control cell for a commercial microscope specify.

This object is achieved with the features of claim 1, advantageous Training can be found in the subclaims relating to this claim 1.

Fig. 1 shows the schematic structure of the temperature control cell designed as a pressure view cell, both in plan and in side view.

The cell is made of martensite-hardenable Ni-Co-Mo steel (Stahlwerk Stahlschmitt GmbH) manufactures and is heated by four heating cartridges (a) (Keller Ihne & Tesch) with a maximum Total power of 200 W. Cooling is carried out by introducing liquid nitrogen into the specially designed cooling channels (b), which are covered by stainless steel cover plates (c) are closed, whereby the chamber temperature is always by an integrated Pt 100 resistor stand (d) is measured.

To determine the sample temperature, however, a special one is placed in the sample space (s) brought and encapsulated against ambient pressure Ni / Cr-Ni thermocouple (f) (SITEC Sieber Engineering AG) used.

Silicone oil AK5 (Wacker Chemie) is used as the pressure medium, via a high-pressure capillary (g) is introduced into the chamber.

The special sample holder plus sample is placed in the sample via the loading opening (h) introduced space (e), after which the loading opening (h) after the Bridgman Principle [4] is sealed.

The pressure-stable viewing window (i), made of sapphire or diamond, is glued to the metal seat (k) using high-temperature adhesive, which in turn is screwed to the chamber using the lock nut (l). A special self-reinforcing metal seal [3] (Gesellschaft für Dichtungstechnik mbH) ensures the necessary tightness (see Fig. 3).

In Fig. 2, a photograph of the pressure view cell, you can also see the electrical connections for heating and Pt 100 as well as the protective covering of the heating cartridges, which are not shown in the schematic representation ( Fig. 1).

The main advantage of the high-pressure viewing cell described - compared to comparable apparatus [1], [2] - is the possibility of simple use as an accessory for a commercial microscope, since the cell can be mounted directly on the microscope stage support using a special holder . (See Fig. 1, 2 and 4)

In this way, examinations in a temperature range of approx. -40 ° C to approx. + 270 ° C under hydrostatic pressures up to approx. 300 MPa possible.

literature

• 1. [1] US 39 69 013
• 2. [2] DD-PS 51 714
• 3. [3] Society for Seal Technology mbH, Dachsbergstr. 33, 7129 Brackenheim; 10 page product overview, received by the Ulm University on 8/26/86
• 4. [4] P.W. Bridgman, The Physics of High Pressure, Bell London (1952)

Reference list

(b) cooling channels
(c) cover plate
(d) Pt 100 of temperature control
(e) sample room
(f) Thermocouple to determine the sample temperature
(g) high pressure capillary
(h) loading for sample installation or removal
(i) Sapphire or diamond windows
(k) window seat
(l) lock nut
(m) Self-reinforcing metal seal
(n) dowel pin
(o) Print media

Claims (4)

1. temperature control cell for heating or cooling a sample to be examined with a microscope,

• 1. with a sample window (e) which has a viewing window (i) and which can be adjusted to a desired temperature by means of electrical heating elements (a) and cooling passages through which coolant flows (b),
• 2. and with a temperature sensor (d) for regulating the temperature of the sample space (e) and a temperature sensor (f) for temperature measurement in the sample space,

characterized by

• 1. that the temperature control cell can be mounted on the sample table or table support of a commercial microscope,
• 2. that the temperature cell is designed to be highly pressure-resistant and for this purpose the viewing window (i) is glued from the inside of the sample space (e) to a window seat (k) secured by lock nuts (l) and sealed via a self-reinforcing metal seal (m)
• 3. and that a sample change without removing the viewing window (i) via a separate, sealable loading opening (h).

2. temperature cell according to claim 1, characterized in that the body of the Temperature cell made of high-strength steel. 3. Temperature control cell according to claim 1 or 2, characterized in that the viewing window (i) a second window is opposite and the two windows are made of sapphire or Diamond exist. 4. temperature control cell according to one of claims 1 to 3, characterized in that, for polarization microscopic examinations of the sample between two crossed Polarizing films can be inserted and together with these via the loading opening can be introduced into the temperature control cell.